CN101116913A - Method for preparing nanocrystalline magnesium alloy powder - Google Patents
Method for preparing nanocrystalline magnesium alloy powder Download PDFInfo
- Publication number
- CN101116913A CN101116913A CNA200710072782XA CN200710072782A CN101116913A CN 101116913 A CN101116913 A CN 101116913A CN A200710072782X A CNA200710072782X A CN A200710072782XA CN 200710072782 A CN200710072782 A CN 200710072782A CN 101116913 A CN101116913 A CN 101116913A
- Authority
- CN
- China
- Prior art keywords
- magnesium alloy
- alloy powder
- hydrogen
- powder
- ball milling
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
A method for preparing nanocrystalline magnesium alloy powder relates to the preparing method of magnesium alloy powder, which solves the problem that the machinery method prepares the powder with long time of ball milling, easy oxidation and low producing efficiency. In the fast solidify method for preparing the powder, only a very few magnesium alloy with exceptive alloy ingredient can obtain the nanocrystalline due to limit by thermodynamics condition. For most of magnesium alloy, crystal grain only can be refined to a range from 1 um to 3 um. The method of the invention is that magnesium alloy ingot is crushed to rough power, the rough power of the first step is put into a goal agate jar, the goal agate jar is vacuum and charged with hydrogen, the rough power is rub with machine in full hydrogen condition and the hydride state nanocrystalline magnesium alloy powder is dehydrogenated in vacuum by heating to get the nanocrystalline magnesium alloy powder material. The invention integrates the hydrogen processing and the machine goal agate method, therefore, the effect of crystal grain refinement is prominent and nanocrystalline is quickly obtained. The invention has the advantages of good thermal stability of hydride state powder, even organization and uneasy oxidation.
Description
Technical field
The present invention relates to the preparation method of magnesium alloy powder.
Background technology
Magnesium alloy is the lightweight structural material of density minimum in the existing metal material, in national defence and national economy key industry fields such as Aero-Space, automobile, communications, has extremely important using value and application prospects.But existing magnesium alloy materials intensity is low, plasticity is poor, makes it be difficult to use as the high-performance light structural material.Therefore, improving the intensity of magnesium alloy materials, improve its plasticity, is the key of expanding the magnesium alloy application and promoting the magnesium alloy industrial development.At present, the method for raising magnesium alloy strength and plasticity mainly contains alloyage process and refined crystalline strengthening method.Adopt to add the alloying means of alloying element, can improve the mechanical property of magnesium alloy, but DeGrain, and alloying element content when high the material preparation difficulty big.Therefore, for magnesium alloy, the refined crystalline strengthening method has more advantage than alloyage process.The method of refined crystalline strengthening magnesium alloy mainly contains: strong strain plastic deformation (SPD) is handled and powder metallurgy process.The magnesium alloy that SPD obtains after handling, its crystallite dimension can't refine to below the 1 μ m.And consider that for the angle of industrial implementation the SPD method has certain degree of difficulty.Powder metallurgy process is the important method of preparation grained material, utilizes powder metallurgy process can prepare various material or products with ultra-fine or nanocrystalline magnesium alloy.Adopting powder metallurgy process to prepare the key issue of ultra-fine crystalline substance, nano-crystal magnesium alloy material, is the nano-crystal magnesium alloy powder of how preparing as the powder metallurgy raw material.At present, the method for preparing nano-crystal magnesium alloy powder mainly contains mechanical alloying and two kinds of methods of rapid solidification: the one, adopt the mechanical alloying method prepare its ball milling time of nano-crystal magnesium alloy powder long, production efficiency is low; The easy oxidation of nano-crystal magnesium alloy powder of mechanical milling process and final preparation on the other hand; The 2nd, quick setting method prepares nano-crystal magnesium alloy powder, owing to be subjected to the restriction of thermodynamic condition, have only the special magnesium alloy of only a few alloying component can obtain nanometer crystal microstructure, for most of magnesium alloys, the employing quick setting method only can be with grain refinement to 1～3 μ m.
Summary of the invention
The present invention proposes a kind of method for preparing nano-crystal magnesium alloy powder, solved following point: one, existingly adopt the mechanical alloying method to prepare long, the easy oxidation of powder of its ball milling time of nano-crystal magnesium alloy powder, production efficiency is low; The 2nd, quick setting method prepares nano-crystal magnesium alloy powder, owing to be subjected to the restriction of thermodynamic condition, have only the special magnesium alloy of only a few alloying component can obtain nanometer crystal microstructure, for most of magnesium alloys, the employing quick setting method only can be with grain refinement to 1～3 μ m.The concrete technical scheme that addresses the above problem is as follows:
The step of method that the present invention prepares nano-crystal magnesium alloy powder is as follows:
Step 1, with weight Mg content be 90～99%, other metal essence is that 1～10% magnesium alloy ingot is broken into meal, the granularity of meal is 1～5mm;
Step 2, the meal material of step 1 is put into ball grinder, ratio of grinding media to material is 60: 1～120: 1, after vacuumizing, charges into the hydrogen of 0.2～1.0Mpa again;
Step 3, carry out mechanical ball milling under the hydrogen condition filling, drum's speed of rotation is 250～400r/min, Hydrogen Vapor Pressure in ball grinder of every interval 1～3h measurement, the variation that guarantees Hydrogen Vapor Pressure in the ball grinder is in the scope of 0.2～1.0Mpa, want hydrogen make-up, ball milling 20～100h when Hydrogen Vapor Pressure is not enough;
Step 4, the hydrogenation state nano-crystal magnesium alloy powder powder that will behind the step 3 ball milling, obtain, under the vacuum condition of 100pa, be heated to 280 ℃～350 ℃ and be incubated 0.5～1h dehydrogenation after, can obtain the nano-crystal magnesium alloy powder material.
The present invention is directed to the existing method deficiency for preparing nano-crystal magnesium alloy powder, combining hydrogen handles and the significant advantage of mechanical ball milling method grain refinement effect, can obtain fast nanocrystalline, also possess simultaneously the hydrogenation state powder thermally-stabilised good, organize the more all even advantages such as oxidation that are difficult for.The invention solves mechanical alloying method easily oxidized problem of magnesium alloy powder when preparing nano-crystal magnesium alloy powder.The nano-crystal magnesium alloy powder of the present invention's preparation, the powder grain size is more tiny, and evenly the crystallite dimension of the hydrogenation state nano-crystal magnesium alloy powder of preparing behind the reaction ball milling is less than 20nm, and the crystallite dimension of nano-crystal magnesium alloy powder is less than 50nm behind the vacuum dehydrogenation.The present invention is suitable for and existing all magnesium alloy materials, do not need the magnesium alloy of special composition, and technology is simple, and the efficient height is energy-conservation and cost is low.
The specific embodiment
The specific embodiment one: the step of the method for present embodiment is as follows:
Step 1, with weight Mg content be 90～99%, other metal essence is that 1～10% magnesium alloy ingot is broken into meal, the granularity of meal is 1～5mm;
Step 2, the meal material of step 1 is put into ball grinder, ratio of grinding media to material is 60: 1～120: 1, vacuumizes, and charges into the hydrogen of 0.2～1.0Mpa;
Step 3, carry out mechanical ball milling under the hydrogen condition filling, drum's speed of rotation is 250～400r/min, Hydrogen Vapor Pressure in ball grinder of every interval 1～3h measurement, the variation that guarantees Hydrogen Vapor Pressure in the ball grinder is in the scope of 0.2～1.0Mpa, charge into purity 〉=99.9% of hydrogen in the ball grinder, when the Hydrogen Vapor Pressure in the ball grinder during less than 0.2Mpa, hydrogen make-up in ball grinder, ball milling 20～100h obtains the hydrogenation state nano-crystal magnesium alloy powder of crystallite dimension less than 20nm;
Step 4, the hydrogenation state nano-crystal magnesium alloy powder powder that will behind the step 3 ball milling, obtain, under the vacuum condition of 100pa, be heated to 280 ℃～350 ℃ and be incubated 0.5～1h dehydrogenation after, can obtain the nano-crystal magnesium alloy powder material.
Its cardinal principle is: utilize the mechanical ball milling under the nitrogen atmosphere to obtain the hydrogenation state magnesium alloy powder of crystallite dimension for 10nm, the magnesium alloy powder with hydrogenation state carries out the vacuum dehydrogenation processing then, obtains the nano-crystal magnesium alloy powder that crystallite dimension is 50nm.
The specific embodiment two: the difference of the present embodiment and the specific embodiment one is that ratio of grinding media to material is 60: 1 in the step 2, and the ball grinder internal pressure is 0.2Mpa, vacuumizes and the number of times that fills hydrogen is 3 times; The step 3 drum's speed of rotation is 250r/min, and the ball milling time is 100h; Vacuum dehydrogenation pressure is less than 100Pa in the step 4, and heating-up temperature is 280 ℃, insulation 1h.Other step is identical with embodiment one.
The specific embodiment three: the difference of the present embodiment and the specific embodiment one is that ratio of grinding media to material is 80: 1 in the step 2, and the ball grinder internal pressure is 0.5Mpa, vacuumizes and the number of times that fills hydrogen is 3 times; The step 3 drum's speed of rotation is 320r/min, and the ball milling time is 60h, and vacuum dehydrogenation pressure is less than 100Pa in the step 4, and heating-up temperature is 310 ℃, insulation 0.75h.Other step is identical with embodiment one.
The specific embodiment four: the difference of the present embodiment and the specific embodiment one is that ratio of grinding media to material is 120: 1 in the step 2, and the ball grinder internal pressure is 1Mpa, vacuumizes and the number of times that fills hydrogen is 3 times; The step 3 drum's speed of rotation is 400r/min, and the ball milling time is 20h; Vacuum dehydrogenation pressure is less than 100Pa in the step 4, and heating-up temperature is 350 ℃, insulation 0.5h.Other step is identical with embodiment one.
Claims (5)
1. method for preparing nano-crystal magnesium alloy powder is characterized in that the step of this method is as follows:
Step 1, with weight Mg content be 90～99%, other metal essence is that 1～10% magnesium alloy ingot is broken into meal, the granularity of meal is 1～5mm;
Step 2, the meal material of step 1 is put into ball grinder, ratio of grinding media to material is 60: 1～120: 1, vacuumizes, and charges into the hydrogen of 0.2～1.0Mpa;
Step 3, carry out mechanical ball milling under the hydrogen condition filling, drum's speed of rotation is 250～400r/min, Hydrogen Vapor Pressure in ball grinder of every interval 1～3h measurement, the variation that guarantees Hydrogen Vapor Pressure in the ball grinder is in the scope of 0.2～1.0Mpa, want hydrogen make-up, ball milling 20～100h when Hydrogen Vapor Pressure is not enough;
Step 4, the hydrogenation state nano-crystal magnesium alloy powder powder that will behind the step 3 ball milling, obtain, under the vacuum condition of 100pa, be heated to 280 ℃～350 ℃ and be incubated 0.5～1h dehydrogenation after, can obtain the nano-crystal magnesium alloy powder material.
2. a kind of method for preparing nano-crystal magnesium alloy powder according to claim 1 is characterized in that charging in the ball grinder purity 〉=99.9% of hydrogen.
3. the method for preparing nano-crystal magnesium alloy powder according to claim 1 is characterized in that ratio of grinding media to material is 60: 1 in the step 2, and the ball grinder internal pressure is 0.2Mpa, vacuumizes and the number of times that fills hydrogen is 3 times; The step 3 drum's speed of rotation is 250r/min, and the ball milling time is 100h; Vacuum dehydrogenation pressure is less than 100Pa in the step 4, and heating-up temperature is 280 ℃, insulation 1h.
4. a kind of method for preparing nano-crystal magnesium alloy powder according to claim 1 is characterized in that ratio of grinding media to material is 80: 1 in the step 2, and the ball grinder internal pressure is 0.5Mpa, vacuumizes and the number of times that fills hydrogen is 3 times; The step 3 drum's speed of rotation is 320r/min, and the ball milling time is 60h, and vacuum dehydrogenation pressure is less than 100Pa in the step 4, and heating-up temperature is 310 ℃, insulation 0.75h.
5. a kind of method for preparing nano-crystal magnesium alloy powder according to claim 1 is characterized in that ratio of grinding media to material is 120: 1 in the step 2, and the ball grinder internal pressure is 1Mpa, vacuumizes and the number of times that fills hydrogen is 3 times; The step 3 drum's speed of rotation is 400r/min, and the ball milling time is 20h; Vacuum dehydrogenation pressure is less than 100Pa in the step 4, and heating-up temperature is 350 ℃, insulation 0.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710072782XA CN101116913A (en) | 2007-09-07 | 2007-09-07 | Method for preparing nanocrystalline magnesium alloy powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710072782XA CN101116913A (en) | 2007-09-07 | 2007-09-07 | Method for preparing nanocrystalline magnesium alloy powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101116913A true CN101116913A (en) | 2008-02-06 |
Family
ID=39053258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200710072782XA Pending CN101116913A (en) | 2007-09-07 | 2007-09-07 | Method for preparing nanocrystalline magnesium alloy powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101116913A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101856722A (en) * | 2010-06-22 | 2010-10-13 | 黑龙江省机械科学研究院 | Method for manufacturing nano-crystal magnesium alloy powder gear |
| CN103752840A (en) * | 2014-01-10 | 2014-04-30 | 太原理工大学 | Quick preparation method of nano magnesium alloy powder |
| CN103922284A (en) * | 2014-03-18 | 2014-07-16 | 哈尔滨工业大学 | AlH3/MgCl2 nanometer complex powder preparation method |
| CN105525119A (en) * | 2014-09-28 | 2016-04-27 | 南京工程学院 | Nanocrystalline magnesium alloy powder consolidation molding preparation method |
| CN105772735A (en) * | 2016-01-19 | 2016-07-20 | 南京工程学院 | Method for preparing nanocrystalline magnesium alloy through mechanical ball milling at room temperature |
| CN108057879A (en) * | 2017-12-21 | 2018-05-22 | 青海大学 | The purifying treatment method and system of a kind of magnesium alloy powder |
| CN109012903A (en) * | 2018-07-20 | 2018-12-18 | 中国科学院长春光学精密机械与物理研究所 | A kind of preparation method of interface disorder nano material |
-
2007
- 2007-09-07 CN CNA200710072782XA patent/CN101116913A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101856722A (en) * | 2010-06-22 | 2010-10-13 | 黑龙江省机械科学研究院 | Method for manufacturing nano-crystal magnesium alloy powder gear |
| CN101856722B (en) * | 2010-06-22 | 2011-08-03 | 黑龙江省机械科学研究院 | Method for manufacturing nano-crystal magnesium alloy powder gear |
| CN103752840A (en) * | 2014-01-10 | 2014-04-30 | 太原理工大学 | Quick preparation method of nano magnesium alloy powder |
| CN103752840B (en) * | 2014-01-10 | 2015-09-16 | 太原理工大学 | A kind of fast preparation method of nanometer Mg alloyed powder |
| CN103922284A (en) * | 2014-03-18 | 2014-07-16 | 哈尔滨工业大学 | AlH3/MgCl2 nanometer complex powder preparation method |
| CN105525119A (en) * | 2014-09-28 | 2016-04-27 | 南京工程学院 | Nanocrystalline magnesium alloy powder consolidation molding preparation method |
| CN105772735A (en) * | 2016-01-19 | 2016-07-20 | 南京工程学院 | Method for preparing nanocrystalline magnesium alloy through mechanical ball milling at room temperature |
| CN108057879A (en) * | 2017-12-21 | 2018-05-22 | 青海大学 | The purifying treatment method and system of a kind of magnesium alloy powder |
| CN109012903A (en) * | 2018-07-20 | 2018-12-18 | 中国科学院长春光学精密机械与物理研究所 | A kind of preparation method of interface disorder nano material |
| CN109012903B (en) * | 2018-07-20 | 2020-05-12 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of surface disordered nano material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101116913A (en) | Method for preparing nanocrystalline magnesium alloy powder | |
| CN100567530C (en) | A kind of preparation method of high performance sinter Mo-Ti-Zr molybdenum alloy | |
| CN104674038B (en) | Alloy material with high strength as well as ductility and semi-solid state sintering preparation method and application of alloy material | |
| CN110484796B (en) | Transition metal carbide high-entropy ceramic particles and preparation method thereof | |
| CN101967591B (en) | Method for preparing Nb3Al superconducting material by mechanical alloying method | |
| CN101279331B (en) | Wire hydrostatic extrusion device and method for extruding superfine crystal grain wire by using same | |
| CN101962724B (en) | Preparation method of Mg-RE-Ni alloy hydrogen storage material | |
| CN100427622C (en) | Preparation method of fine-grained TiAl intermetallic compound material | |
| CN100542949C (en) | The synthetic method of coarse-grain degree cubic boron nitride | |
| CN102277508A (en) | Preparation method of magnesium-based hydrogen storage alloy | |
| CN103331449A (en) | Ultrahigh-plasticity double-size-distribution superfine crystal/micrometer crystal block iron material and preparation method thereof | |
| CN103537688B (en) | A kind of nano-powder prepares the method for Fe-Al alloy | |
| CN102392161A (en) | Aluminum alloy and preparation method thereof | |
| CN104843727B (en) | Multi-component rare earth boride (LaxCe1-x)B6 solid solution polycrystalline cathode material and preparation method thereof | |
| CN103981377B (en) | A kind ofly can improve refining magnesium raw material pelletizing of horizontal tank refining magnesium efficiency and preparation method thereof | |
| CN101693973A (en) | Method and device thereof for preparing Nd-Mg-Ni hydrogen storage alloy by microwave sintering | |
| CN103934453B (en) | Utilize the method for modified metal power forging gasoline engine connecting rod blank | |
| CN103934454A (en) | Manufacturing technology for small gasoline engine connecting rod workblank | |
| CN104232961B (en) | A kind of high-strength height hard Cu-Cr composite and its preparation method and application | |
| CN104593572A (en) | Preparation method of full-density nanocrystalline pure iron block material | |
| CN104402450A (en) | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature | |
| CN107829036A (en) | A kind of powder hot-pressing sintering manufacture method of high silicon steel thin belt material | |
| CN104294070B (en) | A kind of low-temperature sintering preparation is containing the method for Mg aluminium alloy | |
| CN102560167B (en) | Aluminum alloy and preparation method thereof | |
| CN104357738A (en) | Method for preparing Fe-Al alloy from nanometer material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |